Search In this Thesis
   Search In this Thesis  
العنوان
Preparation and analytical applications of copper, manganese and zirconium oxide nanocomposites /
المؤلف
Mahmoud, Nada El-Sayed Marghany.
هيئة الاعداد
باحث / ندى السيد مرغنى محمود
مشرف / مصطفى محمود مصطفى
مناقش / أيمن عوض على عبد الرازق
مناقش / عبدالعظيم محمد الشرقاوى
الموضوع
Inorganic chemistry.
تاريخ النشر
2023.
عدد الصفحات
211 p. :
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
Inorganic Chemistry
تاريخ الإجازة
1/1/2022
مكان الإجازة
جامعة بنها - كلية العلوم - الكيمياء
الفهرس
Only 14 pages are availabe for public view

from 191

from 191

Abstract

The thesis aims to prepare some simple and mixed metal oxides using combustion method and ultrasonication. The prepared simple nanoparticles and mixed nanocomposites were investigated by using different instrumentals. The fabricated simple oxides and their nanocomposites were also used as adsorbents for the removal of organic dye from water.
The thesis consists of three main chapters:
Chapter 1: Introduction
This chapter includes an introduction about water pollution, sources of pollution and its harms on living things, as well as the different methods used to purify polluted water. It also includes the definition of nanomaterials and the different techniques used in their preparation, as well as their applications in different fields. This chapter also includes literature survey on the previous work for the copper, manganese and zirconium oxides and their nanocomposites (ZrO2/Mn2O3 and CuO/Mn2O3) and their applications in various fields such as water treatment.
Chapter 2: Experimental
This chapter contains the practical part of this thesis. It includes the description of the materials and reagents were used in the synthesis of simple and composite. Copper oxide (CuO), manganese oxide (Mn2O3) and zirconium oxide (ZrO2) nanoparticles were synthesized via combustion method using different fuels such as succinic, tartaric and glutamic acids after calcination at 600 ºC for 1h. ZrO2/Mn2O3 and CuO/Mn2O3 nanocomposites were synthesized by the mixing between them in bidistilled water and ultrasonicated for 15 minutes. The obtained nanocomposites were then dried at 100 ºC followed by the calcination at 600 ºC for 10 min.
This chapter includes the description of the instrumental tools which are used in the characterization of the synthesized simple and composite materials such as XRD, FTIR, HR-TEM, FE-SEM, UV-Visible spectra and TGA- DTA. It also contains the explanation for the batch method which used for the removal of organic dye from water using the fabricated adsorbents. It also includes the explanation for various factors influencing the removal efficiency.
Chapter 3: Results and discussion
This chapter contains the discussion and results of the extracted data. It can be divided into two main parts.
Part 1: characterization part
The first part describes the characterization of the obtained copper, manganese and zirconium oxides and ZrO2/Mn2O3 and CuO/Mn2O3 nanocomposites by different tools such as thermal analysis (TG-DTA), powder X-ray (XRD), infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and UV-Vis spectrophotometer.
The extracted data from thermal analysis showed that copper oxide nanoparticles obtained after the calcination in between 350 ºC– 600 ºC. The obtained manganese oxide nanoparticles prepared after the calcination of the ignition ashes at 600 ºC. Also, the synthesized zirconium oxide nanoparticles fabricated after the calcination of the obtained ashes at 600 ºC.
XRD pattern of the calcined copper, manganese and zirconium oxides showed that all samples are in the nanometer range. The crystalline size of the obtained CuO were determined using X-ray and was 41 nm, 23 nm and 26 nm for CGC, CSC and CTC samples, respectively. The crystalline size of manganese oxide determined using X-ray peaks to be 60 nm, 74.3 nm and 30 nm for the MSC, MTC and MGC samples, respectively. The crystalline size of the obtained zirconium oxide determined using X-ray patterns to be 10 nm, 12 nm and 9 nm for the ZGC, ZSC and ZTC samples, respectively. Also, XRD patterns of the obtained copper oxide and manganese oxide nanocomposite showed the presence of CuO and Mn2O3. The average crystalline sizes determined to be 59 nm, 38 nm and 55 nm for all the synthesized nanocomposites MC21, MC11 and MC12, respectively. Also, the synthesized zirconium oxide and manganese oxide nanocomposite showed the presence of ZrO2 and Mn2O3 in the composite. The crystalline sizes determined to be 34 nm, 23 nm and 25 nm for MZ21, MZ11 and MZ12, respectively.
FT-IR spectra appeared peaks at 480 cm-1 and 525-550 cm-1, which related to the copper oxide nanoparticles. Appeared peaks at 420-430 cm-1, 580-590 cm-1 and 680-690 cm-1 are related to the manganese oxide nanoparticles and peaks appeared at 550 cm-1 and 700 cm-1 are related to the zirconium oxide nanoparticles. Also, FT-IR spectra exhibited peaks at 420 cm-1, 500 cm-1, 580-590 cm-1 and 680 cm-1 that related to ZrO2 and Mn2O3 nanocomposites. Also, it exhibited peaks at 450 cm-1, 480 cm-1, 500 cm-1, 520 cm-1 and 660-680 cm-1 that related to CuO and Mn2O3 nanocomposites.
The grain sizes and morphology of the synthesized CuO/Mn2O3 and ZrO2/Mn2O3 nanocomposites studied by using FE-SEM and HR-TEM tools. The morphology of the obtained copper and manganese nanocomposite shows regular and irregular spherical shape. The grain size of CuO/Mn2O3 nanocomposite determined to be 200 nm with hard agglomeration. Also, micrographs of ZrO2/Mn2O3 nanocomposite display the presence of sheets with various hollows. The grain size of ZrO2/Mn2O3 nanocomposite determined to be 85 nm with hard agglomeration.
TEM micrographs of CuO/Mn2O3 nanocomposite show the light and dark irregular spherical shape due to the presence of CuO and Mn2O3 as a mixture in the composite. The particle size of CuO/Mn2O3 determined to be 40 nm and it reflected the presence of hard agglomeration in the synthesized composite. TEM micrographs of ZrO2/Mn2O3 nanocomposite appeared the presence of regular and irregular spherical shape as compact with each other in network shape. The particle size of ZrO2/Mn2O3 nanocomposite determined to be 28 nm with soft agglomeration.
Part2: Application part
The second part includes the adsorption data for the removal of sunset yellow dye using the fabricated Mn2O3, ZrO2/Mn2O3 and CuO/Mn2O3. This part includes the results and discussion of the factors affecting the removal of the dye under study from aqueous solutions such as pH, contact time, initial dye concentration, adsorbent dose, ionic strength and temperature. The optimum conditions for the adsorption process were extracted from the experimental data and the results were as the following:
i. The optimum pH for the adsorption of sunset yellow dye was found to be 2 for the prepared simple oxide Mn2O3 and the nanocomposites ZrO2/Mn2O3 and CuO/Mn2O3.
ii. The contact times for the adsorption of sunset yellow dye using Mn2O3, ZrO2/Mn2O3 and CuO/Mn2O3 samples were found to be 60, 100 and 60 min, respectively.
iii. The amount of dose determined for removal of sunset yellow dye using Mn2O3 and the nanocomposites ZrO2/Mn2O3 and CuO/Mn2O3 to be 50 mg.
iv. The dye removal decreased with increasing the amount of KCl using the synthesized simple and mixed oxides.
v. The dye removal increased with raising the temperature for all the synthesized materials.
vi. The adsorption data followed well the Langmuir isotherm model for all the prepared nanomaterials. The adsorption of the sunset yellow dye fitted the pseudo second order model using all the prepared nanomaterials.
vii. The adsorption of sunset yellow dye showed spontaneous, physiorption and endothermic process for the all adsorbents.
viii. The adsorption capacities of Mn2O3, ZrO2/Mn2O3 and CuO/Mn2O3 samples for removal sunset yellow dye were found to be 160.30, 90.63 and 146.34 mg/g, respectively.